CN102010289B - Method for preparing benzyl bromide - Google Patents
Method for preparing benzyl bromide Download PDFInfo
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- CN102010289B CN102010289B CN 201010261833 CN201010261833A CN102010289B CN 102010289 B CN102010289 B CN 102010289B CN 201010261833 CN201010261833 CN 201010261833 CN 201010261833 A CN201010261833 A CN 201010261833A CN 102010289 B CN102010289 B CN 102010289B
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Abstract
The invention discloses a method for preparing benzyl bromide, comprising the following steps of, in a stirring state, adding 80-150 parts by weight of sulfuric acid with the mass concentration of 95-99 percent, 400-600 parts by weight of benzyl alcohol and 0.5-5 parts by weight of nitrogen-containing or phosphor-containing compound into 800-1500 parts by weight of hydrobromic acid with the mass concentration of 40-55 percent, preserving the heat and reacting for 1-6h at the temperature of 70-100 DEG C, then standing for lamination, extracting an organic layer, then adding water and a sodium carbonate solution with the mass concentration of 1-10 percent into the extracted organic layer liquid, or washing with a sodium bicarbonate solution with the mass concentration of 1-10 percent, standing for lamination, and extracting an organic layer to obtain a crude benzyl bromide product. The method efficiently prevents polymerization of the benzyl bromide in the production process, has high product yield and weak corrosion on equipment and lowers the production cost.
Description
Technical field
The present invention relates to a kind of production method of chemical substance, relate in particular to a kind of method that adopts phenylcarbinol to produce cylite.
Background technology
Cylite is mainly used in organic synthesis and produces whipping agent, the synthetic production method of cylite mainly contains two kinds, a kind of take toluene as raw material, adopt photochemical catalysis, but this route is owing to the generation of a large amount of bromize hydrogen gas, and environmental pollution is serious, severe operational environment, and corrosive equipment increases production cost etc.; Other method is the phenylcarbinol reaction, has the industrial application condition and is easy to control, and product yield is a kind of comparatively desirable synthetic route than advantages of higher, but because cylite is easy to polymerization in process of production, easily causes product yield on the low side.
Summary of the invention
Technical problem to be solved by this invention provide a kind of production cost low, can effectively stop in process of production polymerization of cylite, product yield high, to the method for the light production cylite of equipment corrosion.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of method of producing cylite: under whipped state, be that to add 80～150 weight part mass concentrations in 40～55% the Hydrogen bromide be 95～99% sulfuric acid to 800～1500 weight part mass concentrations, nitrogenous or the phosphorous compound of the phenylcarbinol of 400～600 weight parts and 0.5～5 weight part, 70～100 ℃ of insulation reaction 1～6 hour, then standing demix, extract organic layer, in the organic layer liquid that extracts, add entry afterwards, mass concentration is that 1～10% sodium carbonate solution or mass concentration are 1～10% sodium hydrogen carbonate solution washing, then standing demix, extract organic layer, obtain the cylite crude product.
Be 98% sulfuric acid, the phenylcarbinol of 400～500 weight parts and the nitrogenous or phosphorous compound of 0.5～5 weight part to adding 80～150 weight part mass concentrations during 1000～1500 weight part mass concentrations are 48% Hydrogen bromide preferably.
As the improvement to above-mentioned technology, in described cylite crude product, add the described nitrogenous or phosphorous compound of 0.5～5 weight part, pass through afterwards underpressure distillation and be packaged to be the cylite finished product, the synthesis yield of cylite can reach more than 95%.
As preferred technical scheme, described nitrogenous or phosphorous compound is a kind of or several arbitrarily in triethylamine, DMF, triphenylphosphine or the benzyl triethyl ammonium bromide, can certainly select other can play the additive of same function.
As preferred technical scheme, described extraction organic layer obtains the cylite crude product for extracting the desiccant dryness that directly obtains the cylite crude product behind the organic layer or add capacity in the organic layer liquid that extracts, and obtains the cylite crude product by filtration afterwards.
As preferred technical scheme, described siccative is anhydrous sodium sulphate or anhydrous magnesium sulfate, can certainly select other not with the siccative of organic layer reaction.
Owing to adopted technique scheme, a kind of method of producing cylite: under whipped state, be that to add 80～150 weight part mass concentrations in 40～55% the Hydrogen bromide be 95～99% sulfuric acid to 800～1500 weight part mass concentrations, nitrogenous or the phosphorous compound of the phenylcarbinol of 400～600 weight parts and 0.5～5 weight part, 70～100 ℃ of insulation reaction 1～6 hour, then standing demix, extract organic layer, in the organic layer liquid that extracts, add entry afterwards, mass concentration is that 1～10% sodium carbonate solution or mass concentration are 1～10% sodium hydrogen carbonate solution washing, then standing demix, extract organic layer, obtain the cylite crude product; In process of production polymerization of cylite is made us in the effective prevention of method of the present invention, product yield is high, and light, safe and reliable to equipment corrosion, reduced production cost.
Embodiment
Below in conjunction with embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment one:
Under whipped state, be that to add 80 weight part mass concentrations in 55% Hydrogen bromide be 99% sulfuric acid to 800 weight part mass concentrations, the triethylamine of the phenylcarbinol of 400 weight parts, 0.5 weight part, 70 ℃ of insulation reaction 1 hour, then standing demix extracted organic layer, wash with water to the organic layer liquid that extracts afterwards, then standing demix extracts organic layer, gets the cylite crude product, in the cylite crude product, add 0.5 weight part triphenylphosphine, pass through rectification under vacuum, pack to get the cylite finished product.
The synthesis yield of cylite finished product can reach 95.8%.
Embodiment two:
Under whipped state, be that to add 120 weight part mass concentrations in 48% Hydrogen bromide be 98% sulfuric acid to 1000 weight part mass concentrations, the DMF of the phenylcarbinol of 500 weight parts, 2 weight parts, 90 ℃ of insulation reaction 3 hours, then standing demix, extract organic layer, wash with 8% sodium carbonate solution to the organic layer liquid that extracts afterwards, then standing demix, extract organic layer, get the cylite crude product, add the benzyl triethyl ammonium bromide of 2 weight parts to the cylite crude product, through rectification under vacuum, pack to get the cylite finished product.
The synthesis yield of cylite finished product can reach 95.6%.
Embodiment three:
Under whipped state, add 150 weight part mass concentrations in 1500 weight parts, 40% Hydrogen bromide and be 95% sulfuric acid, the phenylcarbinol of 600 weight parts, 2.5 the triethylamine of weight part, 2.5 the DMF of weight part, 100 ℃ of insulation reaction 6 hours, then standing demix, extract organic layer, using to concentration to the organic layer liquid that extracts afterwards is 10% sodium hydrogen carbonate solution washing, then standing demix, extract organic layer, in the organic layer liquid that extracts, add 100 weight part anhydrous sodium sulfate drying agent, make the cylite crude product by filtration, add the triphenylphosphine of 5 weight parts to the cylite crude product, through rectification under vacuum, pack to get the cylite finished product.
The synthesis yield of cylite finished product can reach 95.9%.
Embodiment four:
Under whipped state, add 120 weight part mass concentrations in 1200 weight parts, 48% Hydrogen bromide and be 97% sulfuric acid, the triphenylphosphine of the phenylcarbinol of 550 weight parts, 3 weight parts, 80 ℃ of insulation reaction 2 hours, then standing demix extracted organic layer, wash with water to the organic layer liquid that extracts afterwards, then standing demix extracts organic layer, gets the cylite crude product, add the triphenylphosphine of 3 weight parts to the cylite crude product, through rectification under vacuum, pack to get the cylite finished product.
The synthesis yield of cylite can reach 95.3%.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
All from the present invention is to devise, the structural transformation of having done without creative work all drops within protection scope of the present invention.
Claims (5)
1. method of producing cylite, it is characterized in that: under whipped state, be that to add 80～150 weight part mass concentrations in 40～55% the Hydrogen bromide be 95～99% sulfuric acid to 800～1500 weight part mass concentrations, nitrogenous or the phosphorous compound of the phenylcarbinol of 400～600 weight parts and 0.5～5 weight part, described nitrogenous or phosphorous compound is triethylamine, DMF, a kind of or several arbitrarily in triphenylphosphine or the benzyl triethyl ammonium bromide, 70～100 ℃ of insulation reaction 1～6 hour, then standing demix, extract organic layer, in the organic layer liquid that extracts, add entry afterwards, mass concentration is that 1～10% sodium carbonate solution or mass concentration are 1～10% sodium hydrogen carbonate solution washing, then standing demix, extract organic layer, obtain the cylite crude product.
2. a kind of method of producing cylite as claimed in claim 1 is characterized in that: be that to add 80～150 weight part mass concentrations in 48% the Hydrogen bromide be 98% sulfuric acid, the phenylcarbinol of 400～500 weight parts and the nitrogenous or phosphorous compound of 0.5～5 weight part to 1000～1500 weight part mass concentrations.
3. a kind of method of producing cylite as claimed in claim 1 is characterized in that: add the described nitrogenous or phosphorous compound of 0.5～5 weight part in described cylite crude product, pass through afterwards underpressure distillation and be packaged to be the cylite finished product.
4. a kind of method of producing cylite as claimed in claim 1, it is characterized in that: described extraction organic layer, obtain the cylite crude product and after extracting organic layer, directly obtain the cylite crude product or in the organic layer liquid that extracts, add desiccant dryness, obtain the cylite crude product by filtration afterwards.
5. a kind of method of producing cylite as claimed in claim 4, it is characterized in that: described siccative is anhydrous sodium sulphate or anhydrous magnesium sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010261833 CN102010289B (en) | 2010-08-20 | 2010-08-20 | Method for preparing benzyl bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010261833 CN102010289B (en) | 2010-08-20 | 2010-08-20 | Method for preparing benzyl bromide |
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| CN102010289A CN102010289A (en) | 2011-04-13 |
| CN102010289B true CN102010289B (en) | 2013-04-03 |
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| CN 201010261833 Active CN102010289B (en) | 2010-08-20 | 2010-08-20 | Method for preparing benzyl bromide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102329192A (en) * | 2011-09-30 | 2012-01-25 | 山东天一化学股份有限公司 | Benzyl bromide synthesis method |
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Address after: 262725 Luyuan Road, Hou Town Industrial Park, Shouguang City, Weifang City, Shandong Province Patentee after: Shandong Luyuan Chemical Technology Co., Ltd. Address before: 262725 Hou Town Industrial Park, Shouguang City, Weifang City, Shandong Province, Luyuan Salinization Co., Ltd. Patentee before: Shouguang Luyuan Salt Chemical Co., Ltd. |
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